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Method for preparing chloroacetic acid by using intermittent chlorination process

A technology of chloroacetic acid and chlorosulfonic acid, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as long reaction time and high content of dichlorine, shorten reaction time, reduce production, and improve reaction efficiency effect

Inactive Publication Date: 2015-04-01
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY +1
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for producing monochloroacetic acid based on intermittent chlorination for the existing intermittent chlorination process, which has long reaction time and relatively high content of dichlorine.

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  • Method for preparing chloroacetic acid by using intermittent chlorination process

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Embodiment 1

[0013] Embodiment 1, a kind of method for producing monochloroacetic acid by intermittent chlorination, its steps are: load weighed acetic acid in the chlorination reactor, then add the main catalyst sulfur whose quality is 1% of the quality of acetic acid successively, the mass The cocatalyst chlorosulfonic acid is 0.5% of the mass of acetic acid, and then the reaction kettle is heated to 70°C, and the circulation pump is started to allow the reaction liquid and chlorine gas in the kettle to enter from the lower end of the 2.5-meter tubular reactor for chlorination reaction. The upper end of the reactor is returned to the reactor, and the reaction time is 0.5 hour. Then, the temperature of the reactor is raised to 100° C., and the reaction liquid and chlorine continue to circulate through the tubular reactor for 6.0 hours to the end.

[0014] After the reaction, the content of monochloroacetic acid was 95.0% and the content of dichloroacetic acid was 1.2% in the product liquid...

Embodiment 2

[0015] Embodiment 2, a kind of method for producing monochloroacetic acid by intermittent chlorination, its steps are: load weighed acetic acid in the chlorination reactor, then add the main catalyst sulfur whose quality is 4% of the acetic acid quality, the mass The cocatalyst chlorosulfonic acid is 0.2% of the mass of acetic acid, and then the reaction kettle is heated to 75°C, and the circulation pump is started to allow the reaction liquid and chlorine gas in the kettle to enter from the lower end of the 3.0-meter tubular reactor for chlorination reaction. The upper end of the reactor is returned to the reactor, and the reaction time is 1.0 hour. Then, the temperature of the reactor is raised to 95° C., and the reaction liquid and chlorine continue to circulate through the tubular reactor for 8.0 hours to the end.

[0016] After the reaction, the content of monochloroacetic acid in the product liquid was 94.8%, and the content of dichloroacetic acid was 1.0%.

Embodiment 3

[0017] Embodiment 3, a kind of method for producing monochloroacetic acid by intermittent chlorination, its steps are: load weighed acetic acid in the chlorination reactor, then add the main catalyst sulfur whose quality is 2.5% of the acetic acid quality, the mass 0.35% chlorosulfonic acid as a co-catalyst of acetic acid quality, then the reaction kettle is heated to 73 ° C, and the circulation pump is started to allow the reaction liquid and chlorine in the kettle to enter from the lower end of the 2.8-meter tubular reactor for chlorination reaction, and then from the The upper end of the tubular reactor was returned to the reactor, and the reaction time was 0.8 hours. Then, the temperature of the reactor was raised to 98° C., and the reaction liquid and chlorine continued to circulate through the tubular reactor for 7.0 hours to the end.

[0018] After the reaction finished, the content of monochloroacetic acid was 95.2% and the content of dichloroacetic acid was 1.1% in the...

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Abstract

The invention discloses a method for preparing monochloro acetic acid based on an intermittent catalytic chlorination process of acetic acid. The method comprises the following steps: sequentially adding acetic acid, a main catalyst which is sulphur and a cocatalyst which is chlorosulfonic acid into a reaction kettle, increasing the temperature of the reaction kettle to 70-75 DEG C, reacting for 0.5-1 hour, then increasing the temperature of the reaction kettle to 95-100 DEG C, and continuously carrying out circulation reaction on a reaction solution and chlorine gas by virtue of a tubular reactor until reaction reaches the final point, wherein the constant temperature of the reaction kettle is retained by the circulation water in the reaction process. The method has the advantages that the production efficiency is high, and the generated dichloroacetic acid is low in content.

Description

technical field [0001] The invention relates to a method for producing chloroacetic acid by intermittent chlorination. Background technique [0002] Chloroacetic acid is an important chemical raw material and intermediate. It has a large market in pesticides, medicines, dyes, organic synthesis, etc., and its development prospects are very broad. At present, the domestic production method of chloroacetic acid mainly adopts acetic acid intermittent catalytic chlorination method, which has long reaction time, low efficiency, unstable product quality and high content of dichloroacetic acid. [0003] In the long run, people have made many improvements to the production of chloroacetic acid. In 1998, Beijing Tsinghua Ziguangyingli Chemical Technology Co., Ltd. proposed to change the distribution mode of chlorine in the Chinese patent "New Process for Chloroacetic Acid Production" with the publication number CN1180066A , using multi-empty multi-tube distributor to increase the con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/16C07C51/363B01J27/02
CPCB01J27/02C07C51/363C07C53/16
Inventor 张向京蒋子超邢宏光胡永琪马连雪高晓洋刘婷婷
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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